反应详情

A mixture of 3-chloro-2,5,6-trifluoro-pyridin-4-ylamine (1.82 g, 10 mmol), 5% Pd/C (0.5 g), and Et3N (3.04 g, 30 mmol) in 50 mL of MeOH was equipped with a balloon of hydrogen gas and stirred at room temperature overnight. The solution was filtered through diatomaceous earth (Celite®). The filtrate was concentrated under vacuum and the residue was partitioned between ethyl acetate and H2O. The aqueous layer was extracted with additional ethyl acetate, and the combined organic layers were washed with brine, dried (MgSO4), filtered and concentrated under vacuum. The residue was purified by flash column chromatography on silica gel with 7:3 hexanes/ethyl acetate to provide 1.33 g (90%) of the desired product. MS (DCI) m/e 149 (M+H)+.

1. filtrationThe solution was filtered through diatomaceous earth (Celite®)
2. concentrationThe filtrate was concentrated under vacuum
3. customthe residue was partitioned between ethyl acetate and H2O
4. extractionThe aqueous layer was extracted with additional ethyl acetate
5. washthe combined organic layers were washed with brine
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated under vacuum
9. customThe residue was purified by flash column chromatography on silica gel with 7:3 hexanes/ethyl acetate